CN111714570A - Separation and purification method of pineapple peel flavone and flavone - Google Patents
Separation and purification method of pineapple peel flavone and flavone Download PDFInfo
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Abstract
The invention belongs to a separation and purification technology of pineapple peel flavone, and particularly relates to a process for separating and purifying pineapple peel flavone by macroporous resin adsorption. The pineapple peel is degreased by using a degreasing agent, then is extracted by using ethanol, and the obtained flavone crude extract is purified by using an optimal scheme. The invention obtains the flavone with higher purity by finding the optimal separation and purification method and adopting the macroporous resin D101 for separation and purification. The recovery rate of flavone obtained by separating and purifying pineapple peel can reach 60.16%, and the purity can reach 86.72%. The antioxidant activity of the purified pineapple peel flavone is stronger than that of unpurified flavone and BHT. Therefore, the pineapple flavone product with high purity and strong oxidation resistance, which is obtained by the invention, provides scientific basis for further industrial production of pineapple peel flavone and improvement of utilization value of pineapple peel.
Description
Technical Field
The invention belongs to a separation and purification technology of pineapple peel flavone, and particularly relates to a separation and purification method of pineapple peel flavone and the flavone.
Background
Pineapple, commonly known as pineapple, is a herbaceous fruit tree of the genus pineapple of the family bromeliaceae, and the fruit is a polymeric fruit consisting of numerous small fruits. The pineapple peel residue accounts for 50-60% of the weight of the whole fruit, wherein the peel accounts for about three, and people usually directly abandon the pineapple peel and only take the pulp for utilization no matter in daily life or factory production. The pineapple peel is similar to the nutrient substances of the pulp, and the waste of the pineapple peel causes great waste of resources. Researches show that the pineapple peel is rich in flavonoids. The flavone is a chemical substance with a plurality of biological activities, has wide application in the aspects of medicine and the like, and has the physiological activities of anticoagulation, blood sugar reduction, tumor resistance, depression resistance, virus resistance, bacteriostasis, in-vivo surplus free radical elimination, aging delay and the like. At home and abroad, the extraction of flavone is reported more, and at present, solvent extraction methods, microwave, ultrasonic waves, enzyme extraction methods and the like are mainly adopted, but the purity of the flavone obtained by the methods is low, so that the effect of the flavone is influenced.
The macroporous resin adsorption method is a purification method widely used in recent years, and has the advantages of good selectivity, no toxicity, no pollution and the like compared with other purification methods, but different macroporous resins have different characteristics and different applicable objects. Therefore, in order to reduce the loss caused by directly discarding the pineapple peels, the invention aims to fully utilize the pineapple peel resources, optimize macroporous resin and process parameters suitable for separating and purifying crude pineapple peel flavone products by using the principle of macroporous resin adsorption after extracting the flavone in the pineapple peel resources in a microwave heating mode, obtain the pineapple flavone products with high purity and strong oxidation resistance, and provide scientific basis for further carrying out industrial production of the pineapple peel flavone and improving the utilization value of the pineapple peels.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention mainly aims to provide a method for separating and purifying the flavone of pineapple peel; the method has the advantages of simple and convenient process, good separation and purification effect and long regeneration and use period.
The invention also aims to provide the pineapple peel flavone prepared by the method.
The technical scheme adopted by the invention for realizing the aim of the invention is as follows:
a method for separating and purifying flavone from pineapple peel comprises the following steps:
step 1, preparation of pineapple peel flavone crude extract
Mixing and degreasing the pineapple peels with a degreasing agent to obtain degreased pineapple peels; then soaking in ethanol solution, and performing microwave heating extraction; carrying out rotary evaporation on the obtained solution to obtain a flavone crude extraction solution;
step 2, separating and purifying the flavone of the pineapple peel
Loading the pretreated macroporous resin into a chromatographic column by a wet method, and adsorbing 0.3-1.5 mg/mL flavone crude extract at the speed of 0.5-2 mL/min; loading the adsorbed macroporous resin into a column by a wet method, and eluting in a chromatographic column by 60-80% ethanol solution at the flow rate of 0.5-2 mL/min; and (4) carrying out rotary evaporation on the obtained eluent to obtain the flavone.
The degreasing agent in the step 1 is at least one of diethyl ether, petroleum ether and ethyl acetate, and preferably petroleum ether.
The solid-liquid ratio of the pineapple peel to the degreasing agent in the step 1 is 1: 1-3 (w/v), and preferably 1:2 (w/v);
the volume fraction of the ethanol solution in the step 1 is preferably 70%; the solid-liquid ratio of the degreased pineapple peels to the ethanol solution is 1: 20-50 (w/v), and preferably 1:30 (w/v).
The soaking time in the step 1 is 4-6 hours; the power during microwave heating extraction is 300-700W, and the extraction time is 5-15 min; preferably, the power for microwave heating extraction is 600W, and the extraction time is 10 min.
The macroporous resin in the step 2 is AB8, D101 or H103, and preferably D101.
The pretreatment process of the resin in the step 2 comprises the following steps: washing the fine resin in the macroporous resin with distilled water, then fully soaking with ethanol, pouring out the immersion liquid, continuously washing the resin with ethanol until the eluate is not turbid when water is added, and then washing with water until no alcohol smell is generated; then, using HCl solution to carry out acid washing on the resin, and then using distilled water to wash the resin to be neutral; then NaOH solution is used for alkali washing, and water washing is carried out until the solution is neutral, thus finishing the treatment.
After the macroporous resin in the step 2 is used for a long time and many times, in order to keep the activity of the resin, the resin is subjected to reinforced regeneration after being used for a period of time, and the method comprises the following steps: adding 3-5% hydrochloric acid solution into a container filled with resin, soaking for 4 hours, then leaching for 3-5 times by using the hydrochloric acid solution with the same concentration, and washing by using distilled water until the solution is nearly neutral. And then soaking the mixture for 4 hours by using a 3-5% sodium hydroxide solution, leaching the mixture for 3-5 times by using the sodium hydroxide solution with the same concentration, and finally washing the mixture to be neutral by using distilled water for later use.
The concentration of the crude flavone extracting solution in the step 2 is preferably 0.6 mg/mL-1.2 mg/mL; the adsorption flow rate is preferably 1 mL/min; the preferred elution flow rate is 1 mL/min-2 mL/min; the volume fraction of the ethanol solution is preferably 65 to 75 percent.
The invention has the beneficial effects that:
1. according to the invention, the D101 macroporous resin is adopted to separate and purify the pineapple peel flavone, the adsorption rate reaches 56.042%, the resolution rate reaches 81.408%, the purity reaches 86.7%, and the purity is remarkably higher than that of the pineapple peel flavone purified by AB8 macroporous resin, namely 35.65%.
2. Compared with the traditional method for preparing the crude flavone extract by directly using ethanol for suction filtration, the method has the advantages that the pineapple peel is degreased by using petroleum ether firstly, then is extracted by using ethanol, and the obtained crude flavone extract is purified by using the optimal scheme. The recovery rate reaches 60.16%, the purity is up to 86.72%, and the invention compares the extraction with petroleum ether and ethanol, and the extraction with ethanol and then petroleum ether, the extraction rate of flavone is increased by 37.98%, the purity of flavone is higher than that of flavone obtained by reported method.
3. The purified flavone obtained by the method has good effects on eliminating DPPH free radicals and hydroxyl free radicals. In the aspect of eliminating DPPH free radicals, the inhibition rate of 0.1mg/mL flavone on DPPH before purification is 90.62%, the inhibition rate of purified flavone on DPPH can reach 93.89%, and the oxidation resistance of the flavone before and after purification is stronger than that of BHT; in the aspect of eliminating hydroxyl radicals, the inhibition rate of 0.1mg/mL flavone on hydroxyl radicals before purification is 70.33%, the inhibition rate on hydroxyl radicals after purification can reach 78.64%, and the antioxidant activity of the flavone before and after purification is stronger than that of BHT (butylated hydroxytoluene), as shown in Table 5.
4. The method for separating and purifying the flavone in the pineapple peel provided by the invention is simple to operate, wide in raw material source, high in recovery rate and high in purity, improves the economic value of the pineapple peel, and is suitable for enterprises and large-scale production.
Detailed Description
The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto. The reagents used in the examples are commercially available without specific reference.
Example 1
A method for separating and purifying flavone from pineapple peel comprises the following steps:
step 1, pineapple peel powder preparation
Cleaning pineapple peel, and drying in a drying oven at 60-70 deg.C. Taking out dried pineapple peel, crushing with a crusher, filling peel powder into a clean sealed bag, and storing in a refrigerator.
Step 2, preparation of pineapple peel flavone crude extract
Accurately weighing a certain amount of dried pineapple peel powder in a 1000mL beaker, degreasing with petroleum ether in a solid-to-liquid ratio of 1:2(W/v), evaporating the petroleum ether to dryness to obtain degreased pineapple peel, soaking in ethanol with a volume fraction of 70% in a solid-to-liquid ratio of 1:30(W/v) for 4-6 h, stirring uniformly, transferring into a 2000mL two-neck flat-bottomed flask, extracting for 10min under a microwave power of 600W, performing suction filtration while hot, transferring into a rotary evaporator, evaporating and concentrating until no ethanol exists, and storing for later use.
Step 3, pretreatment of macroporous resin
Putting a proper amount of D101 macroporous resin into a beaker, washing the resin with distilled water to remove finely-divided resin, fully soaking the resin in 95% ethanol for 24h, pouring out the immersion liquid, continuously washing the resin with 95% ethanol until the eluate is not turbid when water is added, and washing the resin with distilled water until no alcohol smell exists. The resin was acid washed with 5% HCl solution and then washed neutral with distilled water. Then 2% NaOH solution is used for alkali washing, and distilled water is used for washing until the pH value is 7, thus finishing the treatment.
Step 4, separating and purifying the flavone of the pineapple peel
Weighing 20.0g of the pretreated resin, filling the resin into a chromatographic column by a wet method, and adsorbing 1.2mg/mL of 20mL of the crude flavone extract at the speed of 1 mL/min. And (4) measuring the concentration of the flavone in the filtrate after the adsorption is finished, and calculating the adsorption quantity of the flavone. And (3) loading the adsorbed macroporous resin into a column by a wet method, eluting in a chromatographic column by 65% ethanol solution at the flow rate of 1mL/min, and performing rotary evaporation on the obtained eluent to obtain the flavone. After elution, the resin is washed by distilled water until the effluent liquid is colorless and transparent clear liquid, and the absorbance of the eluent is measured.
Example 2
Step 1, pineapple peel powder preparation
Cleaning pineapple peel, and drying in a drying oven at 60-70 deg.C. Taking out dried pineapple peel, crushing with a crusher, filling peel powder into a clean sealed bag, and storing in a refrigerator.
Step 2, preparation of pineapple peel flavone crude extract
Accurately weighing a certain amount of dried pineapple peel powder in a 1000mL beaker, degreasing with petroleum ether in a solid-to-liquid ratio of 1:2(w/v), evaporating the petroleum ether to dryness to obtain degreased pineapple peel, soaking in ethanol with a volume fraction of 70% in a solid-to-liquid ratio of 1:30(w/v) for 4-6 h, stirring uniformly, transferring into a 2000mL two-neck flat-bottomed flask, extracting for 10min under a microwave power of 600w, carrying out suction filtration while hot, transferring into a rotary evaporator, evaporating and concentrating until no ethanol exists, and storing for later use.
Step 3, pretreatment of macroporous resin
Putting a proper amount of D101 macroporous resin into a beaker, washing the resin with distilled water to remove finely-divided resin, fully soaking the resin in 95% ethanol for 24h, pouring out the immersion liquid, continuously washing the resin with 95% ethanol until the eluate is not turbid when water is added, and washing the resin with distilled water until no alcohol smell exists. The resin was acid washed with 5% HCl solution and then washed neutral with distilled water. Then 2% NaOH solution is used for alkali washing, and distilled water is used for washing until the pH value is 7, thus finishing the treatment.
Step 4, separating and purifying the flavone of the pineapple peel
Weighing 20.0g of the pretreated resin, filling the resin into a chromatographic column by a wet method, and adsorbing 1.2mg/mL and 20mL of the crude flavone extract at the speed of 1.5 mL/min. And (4) measuring the concentration of the flavone in the filtrate after the adsorption is finished, and calculating the adsorption quantity of the flavone. Loading the adsorbed macroporous resin into a column by a wet method, eluting with 75% ethanol solution in a chromatographic column at the flow rate of 1.5mg/mL, and performing rotary evaporation on the obtained eluent to obtain the flavone. After elution, the resin is washed by distilled water until the effluent liquid is colorless and transparent clear liquid, and the absorbance of the eluent is measured.
Example 3
Step 1, pineapple peel powder preparation
Cleaning pineapple peel, and drying in a drying oven at 60-70 deg.C. Taking out dried pineapple peel, crushing with a crusher, filling peel powder into a clean sealed bag, and storing in a refrigerator.
Step 2, preparation of pineapple peel flavone crude extract
Accurately weighing a certain amount of dried pineapple peel powder in a 1000mL beaker, degreasing with petroleum ether in a solid-to-liquid ratio of 1:2(w/v), evaporating the petroleum ether to dryness to obtain degreased pineapple peel, soaking in ethanol with a volume fraction of 70% in a solid-to-liquid ratio of 1:30(w/v) for 4-6 h, stirring uniformly, transferring into a 2000mL two-neck flat-bottomed flask, extracting for 10min under a microwave power of 600w, carrying out suction filtration while hot, transferring into a rotary evaporator, evaporating and concentrating until no ethanol exists, and storing for later use.
Step 3, pretreatment of macroporous resin
Putting a proper amount of D101 macroporous resin into a beaker, washing the resin with distilled water to remove finely-divided resin, fully soaking the resin in 95% ethanol for 24h, pouring out the immersion liquid, continuously washing the resin with 95% ethanol until the eluate is not turbid when water is added, and washing the resin with distilled water until no alcohol smell exists. The resin was acid washed with 5% HCl solution and then washed neutral with distilled water. Then 2% NaOH solution is used for alkali washing, and distilled water is used for washing until the pH value is 7, thus finishing the treatment.
Step 4, separating and purifying the flavone of the pineapple peel
Weighing 20.0g of the pretreated resin, filling the resin into a chromatographic column by a wet method, and adsorbing 1.2mg/mL of 20mL of the crude flavone extract at the speed of 2 mL/min. And (4) measuring the concentration of the flavone in the filtrate after the adsorption is finished, and calculating the adsorption quantity of the flavone. Eluting with 70% ethanol solution at flow rate of 2mL/min, and rotary evaporating the eluate to obtain flavone. After elution, the resin is washed by distilled water until the effluent liquid is colorless and transparent clear liquid, and the absorbance of the eluent is measured.
Comparative examples 1 to 2
Comparative examples 1 to 2 differ from example 1 in the type of macroporous resin, specifically shown in table 1, and the measured adsorption and desorption properties thereof are shown in table 2.
Comparative example 3
Comparative example 3 is different from example 1 in the defatting sequence in the flavone extraction process, and the comparative example adopts ethanol extraction, and the obtained filtrate is degreased with petroleum ether in the ratio of 1:1, and the extraction rate is shown in table 3.
Comparative example 4
Comparative example 4 is different from example 1 in that the crude flavone extract was not defatted with petroleum ether.
The differences between the comparative examples 5-12 and the comparative example 4 are that the adsorption flow rate, the elution flow rate and the concentration of the eluent are mixed in different proportions, and the concrete contents are shown in Table 4.
TABLE 1 resins and parameters for separation and purification of pineapple pericarp flavones in example 1 and comparative examples 1-2
TABLE 2 adsorption and desorption performance of different macroporous resins on pineapple peel flavone
Table 2 shows that the H103 resin has a low resolution ratio, the AB8 resin has a low adsorption ratio, and the D101 resin has a moderate adsorption ratio and resolution ratio, so that the D101 macroporous resin is selected as the resin for purifying the pineapple peel flavone.
TABLE 3 Effect of petroleum ether degreasing sequence on pineapple Peel flavone extraction yield
| Pineapple peel powder | Sequence of degreasing | Extraction ratio of flavone (%) |
| Example 1 | Defatting, extracting with ethanol | 2.056 |
| Comparative example 3 | Extracting with ethanol, and defatting | 1.490 |
As can be seen from Table 3, the extraction rate of flavone from the pineapple peel defatted first is 37.98% higher than that of the pineapple peel defatted later, indicating that defatting first is advantageous for improving the extraction rate of flavone, probably because the dry powder has been dehydrated and extracted with petroleum ether to remove some fat-soluble substances, which is advantageous for the penetration of ethanol and the dissolution of flavone components in the later extraction. Meanwhile, the method of degreasing first is adopted, so that the using amount of petroleum ether can be greatly saved, the cost is reduced, and the operation is convenient.
TABLE 4 recovery of pineapple pericarp flavones in examples 1-3 and comparative examples 4-11
As can be seen from Table 4, the crude extract of pineapple peel flavone is degreased by petroleum ether, which significantly improves the recovery rate. Example 1 is the best separation and purification scheme, and after lipid substances are removed by extraction with petroleum ether, the recovery rate of flavone reaches 60.16%, and the purity reaches 86.72%.
The purified pineapple peel flavone can eliminate DPPH free radicals, and the inhibition rate of the purified pineapple peel flavone on hydroxyl free radicals is obviously higher than that before purification, and the specific table is shown in Table 5.
TABLE 5 inhibition rate of scavenging free radical and hydroxyl free radical of flavone solution before and after purification
As can be seen from Table 5, in the aspect of eliminating DPPH free radicals, the antioxidant activity of the purified flavone is stronger than that of the unpurified flavone, and the inhibition rate of the purified flavone on DPPH can reach 94.89%; in the aspect of eliminating hydroxyl free radicals, the antioxidant activity of the purified flavone is stronger than that of unpurified flavone, the inhibition rate of the purified flavone on the hydroxyl free radicals can reach 99.67%, the antioxidant activity of the flavone before and after purification is stronger than that of BHT, and the antioxidant activity of the pineapple peel flavone purified product and the antioxidant activity of BHT are correspondingly enhanced along with the increase of the use concentration.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (9)
1. A method for separating and purifying flavone from pineapple peel is characterized by comprising the following steps:
step 1, preparation of pineapple peel flavone crude extract
Mixing and degreasing the pineapple peels with a degreasing agent to obtain degreased pineapple peels; then soaking in ethanol solution, and performing microwave heating extraction; carrying out rotary evaporation on the obtained solution to obtain a flavone crude extraction solution;
step 2, separating and purifying the flavone of the pineapple peel
Loading the pretreated macroporous resin into a chromatographic column by a wet method, and adsorbing 0.3-1.5 mg/mL flavone crude extract at the speed of 0.5-2 mL/min; loading the adsorbed macroporous resin into a column by a wet method, and eluting in a chromatographic column by 60-80% ethanol solution at the flow rate of 0.5-2 mL/min; and (4) carrying out rotary evaporation on the obtained eluent to obtain the flavone.
2. The method for separating and purifying the pineapple peel flavone as claimed in claim 1, wherein the method comprises the following steps: the degreasing agent in the step 1 is at least one of diethyl ether, petroleum ether and ethyl acetate.
3. The method for separating and purifying the pineapple peel flavone as claimed in claim 1, wherein the method comprises the following steps: the solid-liquid ratio of the pineapple peel to the degreasing agent in the step 1 is 1: 1-3 w/v.
4. The method for separating and purifying the flavone from the pineapple peel according to claim 1, 2 or 3, wherein the method comprises the following steps: the solid-liquid ratio of the degreased pineapple peels to the ethanol solution in the step 1 is 1: 20-50 w/v.
5. The method for separating and purifying the pineapple peel flavone as claimed in claim 1, wherein the method comprises the following steps: the soaking time in the step 1 is 4-6 hours; the power during microwave heating extraction is 300-700W, and the extraction time is 5-15 min.
6. The method for separating and purifying the pineapple peel flavone as claimed in claim 1, wherein the method comprises the following steps: the macroporous resin in the step 2 is AB8, D101 or H103.
7. The method for separating and purifying the pineapple peel flavone as claimed in claim 1, wherein the method comprises the following steps: the pretreatment process of the resin in the step 2 comprises the following steps: washing the fine resin in the macroporous resin with distilled water, then fully soaking with ethanol, pouring out the immersion liquid, continuously washing the resin with ethanol until the eluate is not turbid when water is added, and then washing with water until no alcohol smell is generated; then, using HCl solution to carry out acid washing on the resin, and then using distilled water to wash the resin to be neutral; then NaOH solution is used for alkali washing, and water washing is carried out until the solution is neutral, thus finishing the treatment.
8. The method for separating and purifying the pineapple peel flavone as claimed in claim 1, wherein the method comprises the following steps:
the concentration of the crude flavone extracting solution in the step 2 is 0.6 mg/mL-1.2 mg/mL; the adsorption flow rate is 1 mL/min; the elution flow rate is 1 mL/min; the volume fraction of the ethanol solution is 65-75%.
9. The pineapple peel flavone prepared by the method of any one of claims 1 to 8.
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